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(No Model.) 2 Sheets-Sheeti.

J. VAN RUYMBEKE. PROCESS OF. AND APPARATUS FOR DISTILLING GLYGERIN.

- No. 522,132. Patented June 26, 1894.

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(No Model.) 2 Sheets-Sheet 2.

J. VAN RUYMBEKE. PROGESS OF AND APPARATUS FOR DISTILLING GLYGERIN.

No. 522,132. Patented June 26,1894.

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UNITED STATES PATENT OFFICE.

JOSEPH VAN RUYMBEKE, OF CHICAGO, ILLINOIS, ASSIGNOR OF ONE-HALF Y TO WILLIAM J OBBINS, OF SAME PLACE.

PROCESS OF AND APPARATUSFOR DISTILLING GLYCERI N.

SPECIFICATION forming part of Letters Patent No. 522,132, dated June 26, 1894.

Application filed April 23, 1894.

distillation of easily decomposible material,

and to apparatus therefor. I shall describe this process as it is carried out in the distillation of glycerin, although it is to be understood that it can also be used in distilling other materials liable to be decomposed during distillation, such as oils, fatty acids, 850'.

I shall also describe and claim herein a convenient form of apparatus by means of which my said improved process may be carried out;

but I do not restrict myself to said apparatus or to any apparatus for carrying out the same.

In the accompanying drawings: Figure 1, is a diagrammatic view of a portion of a distilling plant, for the purpose of illustrating my process, and Fig. 2, a side elevation of a convenient form of still and reheater in which the] novel steps of my process can be carried on In both of the above views corresponding parts are designated by the same letters of reference.

Referring to Fig. 1, A represents a still; a, is a heating coil in the'still; b, is an annular distributing pipe, perforated on its under side for injecting steam into the still, such'steam being prepared as I shall presently. point out; B, is a condenser; C, is a receiving tank for the condensed distillate; D, is a vacuum pump; E, is a heating cylinder preferably adjacent to the still; 0, is a steam coil within said heating cylinder, which I shall hereinafter refer to as the expansion coil; d, is a pipe through which steam is admitted to the expansion coil, and which should either be of smaller'diameter than the expansion coil, or else, should be provided with a valve so that the inletopening into the expansion coil may Serial No. 508,694. (NomodeL) source of steam supply with one end of the coil a; h, is a pipe connected with the other end of the coil a, for carryingoff water of condensation from said coil, or, when there is no appreciable condensation, for carrying oft steam from said coil to any point desired; and, h, is a drip pipe for the heating cylinder E.

In Fig. 2, F, F, are heavy standards, four of which are used; G, G, are heavy metal braces bolted to the upper ends of said standards, and H, H, are cross braces, such braces being generally made of ordinary I irons. The still A is supported on said braces G, H, by means of brackets 2'; and the heating cylinder E, is also supported by means of similar brackets at the side of the still. Both the still A, and heating cylinder E are made of boiler iron or steel of sufficient thickness to withstand high pressures.

At the bottom of the still A, is a heavy metal door j, adapted to be bolted in place and packed tightly to prevent leaking. The

said door j, is provided with a draw 'oft pipe is, and a larger draw oft pipe Z, is'generally provided at one side of the said door. Both of said draw ofi pipes 70, Z, are provided with gate valves therein, and by means of said pipes the residue in the still can be drawn oif.

The door j, is used for the purpose of allowing the interior of the still to be reachedfor the purpose of cleaning, .850. the side of the still enables the material which is to be distilled to be introduced therein,

A pi'pe'm, at

said pipe being provided with gate valves which are to be closed when a sufiicient quantity of material has been introduced into the still. A water column a, atthe side 0t the still enables the amount of material therein to be readily determined. At the top ofthe IOO still extends the eduction pipe 0, which leads to the condenser.

p, is a pipe which connects with aboiler or any other suitable source of steam supply, and, q is a four-way casting at the end of said pipe. Extending down from the casting q, midway between the still A, and the reheater E, is a steam pipe 0", provided with an enlarged condensation chamber 8, at its lower end for receiving any water of condensation which may accumulate in the steam pipes 13 or 'r. The condensation chamber is provided with adrip pipe, at its lower end,by means of which the water or condensation may be re- 23', therein, by means of which the amount of 1 steam passing through said pipe may be regu-. lated. It is obvious that the pipe 25, may be.

of the same size as, or even larger than the steam coil 0, and that the valve 15' may yet be so adjusted as to allow the steam to expand in the steam coil as explained. The upper. end ofthe expansion coil connects with a pipe it, which passes out through the wall of the heating cylinder E, and enters thestill A, being connected at its lower end to the annular distributing pipe 1), preferably perforated on its under side as shown. In practice it is desirable that the pipe ushould be of the same or of a larger diameter than the expansion coil so that the steam from the expansion coil may pass freely through the same. Pipe u, is generally provided with a thermometer u, between the still A, and the heating cylinder E, where it may be readily inspected and by means of which the temperature of the injected steam can be determined. Extending out from one of the horizontal portions of the casting q, is a pipe e, which leads into the top of the heating cylinder E, and by means of which the said heating cylinder may be supplied with steam from the boiler. The said pipe 'u, is provided with a valve 11 therein, by means of which the supply of steam to the heating cylinder can be regulated. A drip pipe h, at the lower end of the reheater is provided to draw olf any accumulated water of condensation. Extend ing out from the casting q, is a pipe 00, which passes into the still, and connects with the steam coil a, therein, such pipe being provided with a valve 02 therein, by means of which the supply of steam to the coil a, can be readily regulated. Any water of condensation The object of allowing this which may accumulate in the coil or, may be removed therefrom, throughthe drip pipe h, at the lower end thereof.

In carrying out my process I proceed substantially as follows, attention being particularly directed to Fig. 1 The material to be treated, which is either partly refined glycerin, ora saturated solution of common salt in glycerin, is placed in the still A so as to fill the still to about one-third of its capacity. Steam is now introduced through the pipe f, and passes into and heats the heating cylinder E from which the water of condensation is conducted away by means of the drip pipe h. Steam from the boiler is also passed through the pipe g, and steam coil a, by means of which the material is independently heated during the process of distillation. The steam from the boiler has of course a temperature above that of the boiling point of the material being distilled. To make distillation more rapid and to lower the temperature of distillation a vacuum of about twenty-eight inches should be maintained in the still by the vacuum pump D. Free steam preferably from the same boiler is introduced through the pipe d, into the expansion coil 0, and :by reason of the large size of the latter, this steam will rapidly expand and will consequently suffer a diminution in temperature. Since, however, the expansion coil 0, is heated by free steam in the cylinder E, the expanded steam in said coil will be reheated toabout the temperature of such free steam, or slightly below such temperature. It is obvious that the free steam may be allowed to expand di' rectly into the heating cylinder E, and that it may be reheated by confined steam in a coil within said cylinder. It is further evident that other means for reheating the steam after expansion has taken place, may be used, such as by a steam jacket surrounding the heating cylinder E, or by hot air, or by means of a bath of molten metal having a low melting point, like lead; but in any case it is desirable that the means of reheating the free steam should be such as will prevent material variations in temperature. From the expan sion coil 0, the steam which has been thus expanded and then reheated passes through the pipe 6, and is injected into the material through the perforated distributing pipe Z). This injection of expanded and reheated steam, will rapidly distill the material, and will carrythe distillate over to the condenser B, where it condenses and is caught by the ,plained owing to the large size of the latter.

ing cylinder E, conveyed thereto by the pipe v o. The amount of steam supplied to the heating cylinder maybe adjusted by the valve o, and should be sufficient to reheat the proper amount of expanded steam up to the temperature desired for distillation.

Steam from the pipe 56, enters the steam coil a, and heats the liquid in the still during the distillation.

The particular advantage which properly expanded and reheated steam possesses in distillation is, that the steam expands but slightly and consequently causes but slight absorption of heat due to such expansion. When on the other hand, ordinary free steam is used for distillation, it' always expands very much in the still, and absorbs heat from the contents of the still, so that distillation is retarded not only because of the diminution in temperature thus produced in the material, but also because of the varying quantities of condensed steam retained by the material.

With super-heated steam, that is to say, steam which has been heatedto a high temperature by fire heat or byother means, the same objections are found, and althoughthe diminution in temperature suffered by super-' heated steam in expanding in the still,whether a vacuum is used or not, may not be sufficient to cause condensation, yet such steam is undesirable for the distillation of glycerin or similar materials, since decomposition products will be inevitably formed.

The glycerin prepared as above described may after concentration be again distilled to eliminate the last traces of salts.

Although to obtain the best results, the operation should be carried on in a vacuum, and with means of heatingindependent of the injected expanded and reheated steam, yet to effect the distillation with the omission of either vacuum or the independent means of heating, or both, is also within the scope of my invention, the essence of which consistsin the injection into the glycerin of expanded and reheated steam.

Although the expansion of the steam injected maybe varied within a very wide limit, I have found that steam coming from the boiler at a pressure of from seventy to one hundred and twenty pounds, when expanded to from twenty to thirty times its original volume, will give excellent results.

Although a slight expansion and reheating of the steam to be injected is beneficial pro tcmifo, still it is preferable that the injected steam be expanded until it has a pressure less than that of saturated steam at the boiling point of the liquid from which the glycerin is distilled. To obtain the best results, it is also necessary that the temperature of the in jected steam be kept strictly below the point at which decomposition products are formed. When a high vacuum is used, the pressure of the injected steam may be less than atmos-. pheric pressure.

Having now described my invention, what I claim isi 1. In the art of distilling glycerin and similar liquids the improvement which consists in injecting into the liquid in the presence of a vacuum, steam at less than atmospheric pressure and at a temperature sufficient to effect distillation, substantially as and for the purpose set forth. 1 2. In the art of distilling glycerin or similar liquids,the improvement/which consists in maintaining the liquid to be distilled at a high vacuum, and in injecting expanded and reheated steam into the liquid, as and for the purpose described.

3. In the art of distilling glycerin or similar liquids, the improvement which consists in maintaining the liquid to be distilled at a high vacuum, in independently heating the liquid, and in injecting expanded and reheated steam into the independently heated liquid, main tained at distilling temperature, as and for the purpose described.

4. In the art of distilling glycerin or similar liquids the improvement which consists in maintaining the liquid to be distilled at a high Vacuum, in heating the liquid by means of confined steam, and, in injecting expanded and reheated steam into the heated liquid, maintained at distilling temperature, as and for the purpose described.

5. In the art of distilling glycerin or similar materials, the improvements which consist in maintaining the liquid to be distilled at a high vacuum, in heating the liquid by means of confined steam, in expanding free steam before entering the still, in reheating such I expanded steam by confined live steam of the same temperature as the expanded steam previous to expansion, so as to compensate for reduction of temperature caused by the ex-@ pansion, and in injecting the expanded and reheated steam into the heated liquid maintained at distilling temperature, as and for the purpose described.

6. A distilling apparatus, consisting of a still, an expansion coil, the inlet opening of which is smaller than the outlet opening, a heating cylinder for the expansion coil, and a perforated delivery pipe in the still, and connected with the expansion coil, substantially as described.

7. A distilling apparatus, consisting of a still, a vacuum pump connected with the still, an expansion coil, the inlet opening of which is smaller than the outlet opening, a heating cylinder for the expansion coil, and a perfo .rated delivery pipe in the still and connected with the expansion coil, substantially as de scribed.

8. A distilling apparatus, consisting of a still, a heating coil in the still, an expansion coil, the inlet opening of which is smaller than the outlet opening, a heating cylinder for the expansion coil, and a perforated delivery pipe in the still and connected with the expansion E coil, substantially as described.

9. A distilling apparatus, consisting of a, still, a vacuum pump connected therewith, a heating coil for heating the contents of the still, an expansion coil connected with the still, and with a source of steam supply, the inlet opening of said expansion coil being smaller than the outlet opening, and a heating cylinder for reheating the steam in the expansion coil, substantially as described.

10. A distilling apparatus, consisting of a still, a vacuum pump connected therewith; means for heating the contents of the still;; an expansioncoil connected with the still and i with the boiler, the inlet opening of said expansion coil being smaller than the outlet opening, and a reheater for heating the expansion coil, substantially as described.

11. A distilling apparatus, consisting of a still, a vacuum pump connected therewith, a heating cylinder, an expansion coil in said heating cylinder and connected with the still, 1 the inlet opening of said expansion coil being smaller than the outlet opening, and sources of supply for steam in the said heating cylin- F der and expansion coil, substantially as described.

12. A distilling apparatus, consisting of a: still, a vacuum pump connected therewith, a heating cylinder adjacent to the still and coni nected with a source of steam supply, a heating coil within the still, and an expansion coil in said heating cylinder and connected with the still, the inlet opening of said expansion j coil being smaller than the outlet opening, substantially as described.

13. A distilling apparatus, consisting of a still, a vacuum pump connected therewith, a heating cylinder adjacent to the still and connected with a source of steam supply, a heating coil within the still, connected with the same source of steam supply, a distribut ing pipe within the still, and an expansion coil within the said heating cylinder and connected with said distributing pipe, the inlet opening of said expansion coil being smaller than the outlet opening, substantially as described.

14. A-distilling apparatus, consisting of a still, a vacuum pump connected therewith, a heating cylinder adjacent to the still, connected with a source of steam supply, a heating coil within the still, connected with the same source of steam supply, and an expansion coil within said heating cylinder, connected with the still and supplied withsteam from the same source of steam supply, the inlet opening of said expansion coil being smaller than theoutlet opening, substantially as described.

15. In a distilling apparatus, the combination of the standards F, the braces G and H,

1 bolted to the upper end of the same, the still A and heating cylinder E, supported by said braces, the steam coil (1. within said still, and the expansion coil 0, within said heating cylinder, the inlet opening of said expansion coil being smaller than the outlet opening, substantially as described.

16. In a distilling apparatus, thecombination of the standards F, the braces G and H, bolted to the upper end of the same; the still A and heating cylinder E, supported by said braces, the steam coil a, Within said still, the expansion coil 0 within said heating cylinder, the inlet opening of said expansion coil be ing smaller than the outlet opening, and a common source of steam supply for said steam coil, expansion coil and heating cylinder, substantially as described.

This specification signed and witnessed the 13th day of April, 1894.

JOSEPH VAN RUYMBEKE.

Witnesses:

N. LONGLUND, OHAs. H. OHAPIN. 

